反相流动注射化学发光分析：———QCT—H2O2—Co（Ⅱ）体系测定 …

采用反相流动注射分析方法研究了ＱＣＴ－Ｈ２Ｏ２－Ｃｏ（Ⅱ）化学发光体系,并用于天然水中微量钴的测定,方法的线性范围为０．２￣７０ｎｇ·ｍｌ＾－１,检出限为０．０１ｎｇ·ｍｌ＾－１,九次连续测定的标准偏差为１．６％。     

催化动力学光度法测定痕量Cr（Ⅲ）

在弱酸性介质中,以２,２‘－联吡啶作活化剂,Ｃｒ（Ⅲ）强烈论过氧化氢氧化中性红褪色反应,催化反应的表观活化能为４９．８８ｋＪ·ｍｏｌ＾－１。据此建立了测定痕量Ｃｒ（Ⅲ）的催化动力学光度法。方法的检出限为２ｎｇ·ｍｌ＾－１,线性范围为０￣０．１μｇ·ｍｌ＾－１。通过测定模拟 １、矿井水样及电镀废水样中痕量Ｃｒ（Ⅲ）,结果满意。     

溶剂浮选光度法测定痕量铜

提出了利用溶剂浮选富集ＤＤＴＣ－Ｃｕ（Ⅱ）体系测定水样中痕量铜的方法（ＤＤＴＣ为二乙胺二硫代甲酸钠）。质量浓度的检出限为０．０５ｎｇ·ｍＬ＾－１,线性范围为０．０￣６．０ｎｇ·ｍＬ＾－１,测定含Ｃｕ（Ⅱ）４．０ｎｇ·ｍＬ＾－１的样品,相对标准偏差为０．８５％,已用于天然水中Ｃｕ（Ⅱ）的测定。     

壳聚糖修饰电极开路富集测定工业废水中铅

通过共价键合的方式，制成壳聚糖修饰电极，建立了在非电解条件下，壳聚糖修饰电极络合富集测定Ｐｂ（Ⅱ）的方法，同时对壳聚糖修饰电极的作用机理进行了探讨。Ｐｂ（Ⅱ）的线性范围为０．５０￣２００μｇ·ｍｌ＾－１，相对标准偏差为７．９％，定量下限为０．５０μｇ·ｍｌ＾－１，方法的回收率为９４％￣１０５％。     

单扫示波极谱法测定溴离子

在０．４５ｍｏｌ·Ｌ＾－１硝酸底液中,用单扫示波极谱仪,阳极化扫描,导数档,溴离子于＋０．１４Ｖ产生一尖锐、灵敏的极谱波。检出限为２μｇ·ｍｌ＾－１,工作曲线由２．４￣１０μｇ·ｍｌ＾－１及１０￣２０μｇ·ｍｌ＾－１两条不同斜率的直线组成,前者灵敏度是近者的两倍。常见阳离子Ｆ＾－、ＳＯ４＾２－、ＢｒＯ＾－３、ＮＯ３＾－不干扰Ｂｂ＾－的测定,用此法测定长江水、溴酸钾中的微量溴离子,回收率为１０７％和     

胶束增敏荧光光度法测定布美他尼

提出了在表面活性剂ＴｒｉｔｏｎＸ－１００存在下,高灵敏度胶束增敏测定布美他尼的荧光光度新方法。方法灵敏度高,检出限为２．０·１０＾－８ｍｏｌ·Ｌ＾－１,线性范围宽,为２．２·１０＾－８￣１．５·１０＾－５ｍｏｌ·Ｌ＾－１回收率为９９．８％,本对测定条件作了详细研究,本方法已应用于样品中布美他尼的测定。     

在OP存在下亮甲酚蓝吸光光度法间接测定铵的研究

用氢氧化钠碱解馏分离出氨，以亮甲酚蓝为显色剂，采用吸光光度法进行了铵的间接测定，非离子表面活性剂ＯＰ具有胶束增溶作用；方法的检测波长为５２０ｎｍ，检出限和线性范围分别为０．０５μｇ·ｍｌ＾－１和０．０５￣１．３μｇ·ｍｌ＾－１。将方法分别用于土壤及水样中铵的测定，结果令人满意。     

流动注射在线螯合树脂预富集火焰原子吸收光谱法测定 …

研究了以国产Ｄ４１２螯合树脂作柱材料的流动注射在线微柱预富集火焰原子吸收光谱法测定铜的方法。选择了最佳的富集条件,在富集时间６０ｓ时,富集４６倍,检出限为０．４ｎｇ·ｍｌ＾－１（３σ）,ＲＳＤ为１．６％（２０ｎｇ·ｍｌ＾－１Ｃｕ,ｎ＝１１）分析速度为３０次·ｈ＾－１。并用此法进行水中痕量铜的测定。     

氟化钙增敏石墨炉原子吸收法测定人发和血清样品中痕量钼的研究

石墨炉原子吸收法测定生物样品中痕量钼时，用氟化钙作基体改进剂，可使钼的原子吸光度提高５．７倍，其特征量原来的４．２× １０＾－１１ｇ／１％吸收降低到５．１×１０＾－１２ｇ／１％吸收，测定下限为０．５５ｎｇ·ｍＬ＾－１，线性范围为０～１０００ｎｇ· ｍＬ＾－１． 对人发和牛血清标样中痕量钼测定。结果满意。     

流动注射—结晶紫—磷钼杂多酸离子缔合体系光度法测定水中痕？…

在一定的酸度条件下，结晶紫与磷钼杂多酸离子缔合物的流动注射分光光度法可直接测定痕量磷。灵敏度高，重现性和选择性好。水中常见离子不干扰痕量磷的测定，工作曲线的线性范围为０￣５００μｇ·Ｌ＾－１的磷，检出下限达１．０μｇ·Ｌ＾－１，以１２０ｈ＾－１采样频率，对各种天然水样进行测定，回收率为９２．５％￣１０５．０％，相对标准偏差为０．１％￣６．７％。     

Cu(Ⅱ)-抗坏血酸-三氯偶氮胂体系催化动力学光度法测定痕量铜的研究

在乙酸-乙酸钠缓冲溶液(pH4.4)中,以Cu(Ⅱ)催化抗坏血酸还原三氯偶氮胂褪色为指示反应,建立了测定痕量Cu(Ⅱ)的新方法.测定了反应级数和表观活化能.在70℃水浴中加热6min,测定的灵敏度为3.1×10~(-12)g·ml~(-1),线性范围为0～70ng/25ml.用于测定几种中草药样品中的铜,结果满意,相对标准偏差小于3%.     

铜催化抗坏血酸还原酸性铬深蓝动力学光度法测定痕量铜

在乙酸-乙酸钠介质中,以邻菲罗啉为活化剂,铜对抗坏血酸还原酸性铬深蓝具有强烈的催化作用,测定了反应的表观活化能,探讨了反应机理,建立了测定痕量铜的催化动力学新方法,测定的线性范围为2.5～60ng·ml~(-1),直接用于食品及人发中铜的测定。结果满意。     

溴酸钾氧化酸性铬深蓝催化动力学极谱法测定痕量钒

在0.15mol·L~(-1)H_2SO_4介质中,以酒石酸作活化剂,Ⅴ(Ⅴ)对溴酸钾氧化酸性铬深蓝的反应具有强烈的催化作用,以极谱法监测催化反应过程中酸性铬深蓝浓度的变化,建立了测定痕量钒的催化动力学新方法。钒的线性范围为0.10～7.0ng·ml~(-1),检出限为0.05ng·ml~(-1),应用于人发中痕量钒的测定,结果满意。并对酸性铬深蓝的极谱特性进行了初步的探讨。     

Spectrofluorimetric method for determination of aluminium with chromotropic acid and its application to water samples

A rapid and sensitive method for the trace level determination of aluminium based on the formation of a 1:1 complex with chromotropic acid (1,8-dihydroxynaphthlene-3,6-disulfonic acid) in an methanol medium is reported. The fluorescence intensity of the system was 50 times greater than that of the system without aluminium. This method is very sensitive and selective for the direct determination of aluminium ion. The fluorescence is excited at 346 nm and measured at 370 nm. The optimum conditions are a chromotropic acid concentration of 5.0 ml (1.0x10(-4) M) and pH 4.0+/-0.5 (acetic acid-sodium acetate buffer). The fluorescence intensity is a linear function of the concentration of Al(III) in the range 2-100 ng ml(-1) and the detection limit is 1.0 ng ml(-1). The method has been applied successfully to the determination of trace amount of Al(III) in tap, river and sea-water samples.     

2,6-Bis[(o-hydroxy)phenyliminomethyl]-1-hydroxybenzene as a reagent for the selective spectrofluorimetric determination of aluminium

A spectrofluorimetric method for the determination of aluminium at ng/ml level has been developed. The method is based on the formation of a fluorescent 11 complex between Al(III) and 2,6-bis[(o-hydroxy)phenyliminomethyl]-1-hydroxybenzene at an apparent pH of 5.0 in an aqueous-ethanol medium (70% v/v ethanol). The influence of reaction variables is discussed. The range of concentration of the method is 1.0–10.0 ng/ml aluminium, the relative standard deviation 1.5% and the limit of detection 0.1 ng/ml. The advantages of the proposed method include high sensitivity and selectivity. The method has been applied to the determination of aluminium in natural waters.     

石墨探针—原子吸收光谱法测定人发中痕量铟的研究

探针原子化技术是一种实现等温原子化,改善灵敏度的行之有效的方法。本文采用此方法对痕量钿进行了一系列条件试验,峰面积与钿浓度在0～50ng·ml~(-1)范围内呈线性关系,其特征量4.8pg,检出限21.5pg,相对标准偏差5.7％,并成功地测定了成人发中铟的含量,范围在12～159pg·g~(-1),回收率96.4％～103.2％。该方法灵敏度高,操作简单、快速,结果满意。     

Simultaneous determination of beryllium and aluminium in mixtures using derivative spectrophotometry

The spectrophotometric determination of beryllium and aluminium with 5,8-dihydroxy-1,4-naphthoquinone in the presence of a non-ionic surfactant is reported. Absorption maxima, molar absorptivity and Sandell's Sensitivity of 1:2 (M:L) beryllium and aluminium complexes are, 585 nm and 598 nm, 1.63 x 10(4) l.mole(-1).cm(-1) and 2.04 x 10(4) l.mole(-1).cm(-1), and 0.55 ng/cm(2) and 1.32 ng/cm(2) respectively. Beer's law is obeyed between 7.20-3.96 x 10(2) ng/ml beryllium and 1.08 x 10(1)-1.08 x 10(3) ng/ml aluminium. A method for simultaneous determination of beryllium and aluminium in their mixture using derivative spectra is described. The range 3.6 x 10(1)-3.6 x 10(2) ng/ml beryllium could be determined in the presence of 1.08 x 10(2)-1.08 x 10(3) ng/ml aluminium, and vice versa.     

Differential pulse cathodic stripping adsorption voltammetric determination of trace amounts of lead using factorial design for optimization

A sensitive cathodic stripping voltammetric method is developed for determination of lead(II), with adsorptive collection of complexes with Pyrogallol red (PGR) on to a hanging mercury drop electrode. After accumulation of the complex at −0.80 V vs. Ag/AgCl reference electrode, the potential is scanned in a negative direction from −0.20 to −0.50 V with differential pulse method. Then the reduction peak current for the lead(II)-PGR complex is measured at −0.39 V. The influence of reagent and instrumental variables was completely studied by factorial design analysis. The optimum analytical conditions for the determination of lead(II) were established. Under optimum conditions, lead(II) determined in the range of 0.1-30.0 ng ml⁻¹ with a limit of detection of 0.06 ng ml⁻¹. The method is successfully applied to determination of lead(II) in water sample.     

Separation and determination of trace amounts of aluminium(III), vanadium(V), iron(III), copper(II) and nickel(II) with CALKS and PAR by RP-HPLC.

An RP-HPLC method for the separation and determination of aluminium(III), vanadium(V), iron(III), copper(II) and nickel(II) with CALKS (Chromazol KS) and PAR ([4-(2-pyridylazo)resorcinol]) chelating on a YWG-ODS column was developed. A mixture of methanol-tetrahydrofuran(THF)-water (60:5:35 v/v) containing 0.2 mol/L LiCl, 5 x 10(-5) mol/L CALKS, 5 x 10(-5) mol/L PAR and acetate buffer solution (pH 4.9) was selected as mobile phase. The method has high sensitivity, with the detection limits being 6 ng/mL for aluminium(III), 3.5 ng/mL for vanadium(V), 10.4 ng/mL for iron(III), 6.3 ng/mL for copper(II) and 8.7 ng/mL for nickel(II). It also has good selectivity, so that most foreign metal ions do not interfere under the optimum conditions. The method can be applied to the simultaneous determination of trace amounts of aluminium, vanadium, iron, copper and nickel in rice and flour samples.     

Simultaneous determination of copper, bismuth and lead by adsorptive stripping voltammetry in the presence of thymolphthalexone.

A novel, sensitive and selective adsorptive stripping procedure for simultaneous determination of copper, bismuth and lead is presented. The method is based on the adsorptive accumulation of thymolphthalexone (TPN) complexes of these elements onto a hanging mercury drop electrode, followed by reduction of adsorbed species by voltammetric scan using differential pulse modulation. The influences of control variables on the sensitivity of the proposed method for the simultaneous determination of copper, lead and bismuth were studied using the Derringer desirability function. The optimum analytical conditions were found to be TPN concentration of 4.0 microM, pH of 9.0, and accumulation potential at -800 mV vs. Ag/AgCl with an accumulation time of 80 s. The peak currents are proportional to the concentration of copper, bismuth and lead over the 0.4-300, 1-200 and 1-100 ng mL(-1) ranges with detection limits of 0.4, 0.8 and 0.7 ng mL(-1), respectively. The procedure was applied to the simultaneous determination of copper, bismuth and lead in the tap water and some synthetic samples with satisfactory results.